HRID238618

反应详情

EQUATION

反应方程式

HRID 238618 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of (4-benzyloxy-1-bromo-6-fluoro-naphthalen-2-yl)-acetic acid methyl ester (400 mg, 0.992 mmol) in ethyl acetate (10 mL) was added zinc bromide (670 mg, 2.978 mmol) and 10% palladium on carbon (40 mg) under a hydrogen atmosphere (balloon). After being stirred at room temperature for 1 hour, the resulting mixture was filtered. The filtrate was concentrated in vacuo. The residue was purified by preparative HPLC (gradient elution with 50-80% 0.1% trifluoroacetic acid in water in acetonitrile, 8 minutes) to afford (1-bromo-6-fluoro-4-hydroxy-naphthalen-2-yl)acetic acid methyl ester (200 mg, 64.4%) as a white solid.

WORKUP

后处理

  1. filtrationthe resulting mixture was filtered
  2. concentrationThe filtrate was concentrated in vacuo
  3. customThe residue was purified by preparative HPLC (gradient elution with 50-80% 0.1% trifluoroacetic acid in water in acetonitrile, 8 minutes)